连续反应-萃取耦合技术制备硫酸羟胺  

Preparation of hydroxylamine sulfate by continuous reaction-extraction coupling technology

作　　者：彭超 王榆元[1] 邓昌爱[1] 赵方方[2] 游奎一[2] PENG Chao;WANG Yuyuan;DENG Chang′ai;ZHAO Fangfang;YOU Kuiyi(College of Chemistry and Chemical Engineering, University of South China, Hengyang 421001, Hunan, China;College of Chemical Engineering, Xiangtan University, Xiangtan 411105, Hunan, China)

机构地区：[1]南华大学化学化工学院,湖南衡阳421001 [2]湘潭大学化工学院,湖南湘潭411105

出　　处：《化工学报》2019年第5期1842-1847,共6页CIESC Journal

基　　金：湖南省教育厅科研项目(14C1004);湖南省教育厅一般项目(16C1539);国家自然科学基金青年科学基金项目(21606186)

摘　　要：以环己酮肟和硫酸为原料,研究连续反应-萃取耦合技术条件下环己酮肟水解制备硫酸羟胺。通过优化连续反应-萃取条件,将水解得到的另一产物环己酮从原有平衡体系分离,突破原反应平衡的限制,极大提高环己酮肟的转化率。结果表明,在以环己烷作为萃取剂,酸肟比1∶1,转速为2000～2500 r/min,硫酸溶液与环己烷等体积比的条件下,反应条件最佳。同时测得当原料从重相进料,通过五级串联逆流反应萃取,90 min反应基本达到平衡,经过四次循环萃取后环己酮肟转化率可达81.90%。Using cyclohexanone oxime and sulfuric acid as raw materials, the hydrolysis of cyclohexanone oxime under continuous reaction-extraction coupling technology was studied to prepare hydroxylamine sulfate. The continuous reaction-extraction conditions were optimized. Cyclohexanone which as another product of hydrolysis reaction was separated from the original reaction equilibrium. This technology broke through the limits of the original reaction equilibrium, it greatly improved the conversion rate of cyclohexanone oxime. The results showed that the best reaction conditions were: cyclohexane used as the extraction agent, the ratio of oxime to acid 1∶1, the rotational speed 2000-2500 r/min, and the volume ratio of sulfuric acid solution to cyclohexane 1∶1. At the same time, when the raw material was fed from the heavy phase and extracted by five-stage series countercurrent reaction, after 90 min, the reaction basically reached equilibrium. After four cycles of extraction, the conversion rate of cyclohexanone oxime could reach 81.90%.

关 键 词：反应-萃取耦合 反应 平衡 水解 环己酮肟 硫酸羟胺 

分 类 号：TQ028[化学工程]